CN112144011A - Method for preparing anti-oxidation coating on surface of molybdenum and molybdenum alloy protection tube - Google Patents
Method for preparing anti-oxidation coating on surface of molybdenum and molybdenum alloy protection tube Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/78—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes more than one element being applied in more than one step
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
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Abstract
The invention relates to a method for preparing an antioxidant coating on the surface of a molybdenum and molybdenum alloy protection tube, which prepares a titanium modified molybdenum silicide coating by using an embedding infiltration method, optimizes the relationship between the type selection of a dispersing agent, the quality of an embedding infiltration mixed material and the surface area of a sample, and improves the deposition efficiency. The molybdenum and the molybdenum alloy protection pipe prepared by the method are continuously oxidized for 180 hours under the periodic cyclic oxidation environment of 1200 ℃, obvious weight loss does not occur, and the coating can play an anti-oxidation effect on the molybdenum and the molybdenum alloy protection pipe.
Description
Technical Field
The invention relates to a metal surface treatment method, in particular to a method for preparing an antioxidant coating on the surface of a molybdenum and molybdenum alloy protection tube.
Background
The molybdenum tube prepared after thermoplastic processing has good high-temperature air tightness and can meet the test requirement of the tungsten-rhenium thermocouple wire in an atmosphere protection furnace. However, molybdenum has poor oxidation resistance, which limits the use of molybdenum protective tubes in oxidizing atmospheres.
The preparation of the oxidation resistant coating on the surface of the molybdenum and the molybdenum alloy is a main idea for enabling the molybdenum and the molybdenum alloy to have oxidation resistance at high temperature. Currently, the use of molybdenum-based silicide coatings is most prevalent because of the dense SiO formed on the coating surface as the silicide oxidizes2The layer can prevent oxygen from diffusing into the matrix and avoid direct contact of oxygen with the matrix for oxidation. Simultaneously, SiO is formed2The coating is a glass phase, has good fluidity at high temperature, and can make up for the defects of cracks, holes and the like generated by factors such as thermal expansion and the like in the oxidation process of the coating. The preparation of silicide coating on the surface of molybdenum comprises the methods of thermal spraying, embedding infiltration, chemical vapor deposition, slurry brush coating and the like, wherein the method for preparing single siliconized coating on the surface of molybdenum is disclosed in the structure of preparing molybdenum silicide coating on molybdenum substrate by molten salt method, and Si, NaF, Na and the like are utilized2SiF6、Al2O3The coatings prepared for the mixtures are stable to oxidation for 100h in static air at 1200 ℃ (xieping, mechanical engineering material 2012, 36(001): 65-67). However, the single siliconizing coating has certain limitations, such as the brittleness of the coating at the temperature lower than 1000 ℃ and the poor strength and creep resistance at the temperature higher than 1250 ℃, for example, when the protection tube for the thermocouple is used, the coating of the protection tube cracks once cooled and can not be used, namely, the coating of the protection tube is easy to crack and fail under the condition of cyclic oxidation.
The embedding infiltration method has the advantages of high bonding strength between the coating and the matrix, simple process, no limitation of the size and shape of a sample and the like. However, the coating obtained by the current embedding infiltration method has single component, and still cannot solve the problems that the coating is easy to crack and has short service life under the periodic oxidation environment.
Disclosure of Invention
The invention aims to provide a method for preparing an antioxidant coating on the surface of a molybdenum and molybdenum alloy protection pipe. The method of the invention prepares the titanium modified molybdenum silicide coating by using the pack cementation method, optimizes the relationship between the dispersant type selection and the pack cementation quality and the sample surface area, and improves the deposition efficiency. The molybdenum and the molybdenum alloy protection tube prepared by the method have the advantages that under the periodic cyclic oxidation environment of 1200 ℃ (the temperature is raised to 1200 ℃ and kept for 10 hours, and then is reduced to the room temperature, so that the cyclic oxidation environment is a cycle), the cyclic oxidation is continued for 180 hours, the obvious weight loss is not generated, the cyclic oxidation protection tube is obviously superior to the protection life of the previous single siliconizing coating which is stably oxidized for 100 hours under the static oxidation environment of 1200 ℃ (the temperature is kept after being stably raised to 1200 ℃, and the temperature is not changed any more), and the oxidation resistance of the molybdenum and the molybdenum alloy protection tube can be obviously improved by the oxidation resistant coating.
The technical scheme of the invention is as follows:
a method for preparing an antioxidant coating on the surface of a molybdenum and molybdenum alloy protection tube comprises the following steps:
1) cleaning of
Putting the protection tube into 5 wt% NaOH solution, ultrasonically cleaning, then ultrasonically cleaning the protection tube in alcohol and distilled water in sequence, and drying;
2) end enclosure treatment of protective tube
Welding one end of the protection tube by using cylindrical molybdenum block argon arc welding, and then cleaning by using the method in the step 1) to obtain a matrix to be infiltrated;
3) preparation of the powder to be infiltrated 1
According to the weight of Ti powder: SiO 22Powder (weight): NH (NH)4F (volume) is 40:50:10, and the materials are mixed and ball-milled for 2 hours to obtain powder 1 to be infiltrated;
wherein the total mass m of the mixture is more than or equal to m0·SInner part+m1SOuter cover，
In the formula, m0、m1The embedding permeability coefficient represents the mass of the mixture required by the unit surface area of the matrix, and the outer surface m1＝3g/cm2Inner surface m0＝0.24g/cm2，SInner part、SOuter coverThe inner and outer surface areas of the substrate contacted with the embedded seeping material respectively;
4) heat treatment for infiltration into earth 1
Injecting the powder material 1 to be infiltrated into a protection tube, placing the protection tube in a crucible and embedding the powder material 1 to be infiltrated, sealing the crucible, heating to 1000 ℃ under the argon condition, preserving the heat for 5 hours, and then cooling to room temperature to obtain a secondary coating layer;
5) surface treatment of pipes
Taking out the powder in the protection tube, immersing the protection tube in an alcohol solution, and drying after ultrasonic cleaning;
6) preparation of the powder to be infiltrated 2
According to Si powder (weight): SiO 22Powder (weight): NH (NH)4F (weight) 40:50:10, and performing ball milling and mixing for 2 hours to obtain powder 2 to be infiltrated;
wherein the total mass of the buried infiltration material of the powder 2 to be infiltrated meets the condition that m is more than or equal to m0·SInner part+m1SOuter cover，
In the formula, m0、m1The embedding permeability coefficient represents the mass of the mixture required by the unit surface area of the matrix, and the outer surface m1＝2.5g/cm2Inner surface m0＝0.18g/cm2，SInner part、SOuter coverThe inner and outer surface areas of the substrate contacted with the embedded seeping material respectively;
7) burying and infiltrating heat treatment 2
Repeating the step 4), wherein under the argon condition, the temperature is raised to 1100 ℃, the temperature is kept for 5 hours, and then the coating is cooled to the room temperature to obtain the coating outer layer;
repeat step 5).
The outer layer of the coating is (Mo, Ti) Si2Layer, the secondary outer layer is MoSi2Mo is between the layer, the coating and the substrate5Si3And a transition layer.
The thickness of the outer layer is 5-20 mu m, the thickness of the secondary outer layer is 40-70 mu m, and the thickness of the transition layer is 5-30 mu m.
The molybdenum block in the step 2) is a cylindrical molybdenum block with the same inner diameter as the pipe.
The welding current in the step 2) is 50-150A, and the argon flow is 15 ml/min.
The invention has the technical effects that:
1. the titanium modified molybdenum silicide coating is prepared by using the embedding and permeating method, the relation between the type selection of the dispersing agent, the quality of the embedding and permeating mixture and the surface area of a sample is optimized, and the deposition efficiency is improved. The coating prepared by the method comprises a 3-layer structure and outer layers (Mo, Ti) Si which are continuously distributed2Layer, sub-outer layer MoSi2Mo is between the layer, the oxidation resistant layer and the substrate5Si3And a transition layer.
2. The molybdenum and the molybdenum alloy protection tube prepared by the method have no obvious weight loss after continuous oxidation for 180 hours in a 1200 ℃ periodic cyclic oxidation environment, and have obvious anti-oxidation effect on the molybdenum and the molybdenum alloy protection tube.
3. The protection tube with the blind end is manufactured by welding the molybdenum blocks, and the anti-oxidation coating is manufactured on the inner surface and the outer surface of the molybdenum and the alloy protection tube by using the buried infiltration method, so that the structure of the molybdenum and the alloy protection tube is optimized, and the application range of the molybdenum and the alloy protection tube under the high-temperature oxidation atmosphere is widened.
The coating prepared by the method is (Mo, Ti) Si2-MoSi2-Mo5Si3The composite coating system improves the oxidation resistance of the molybdenum and the molybdenum alloy protection pipe in a periodic oxidation environment, and solves the problems that a single coating is easy to crack and short in service life in the periodic oxidation environment.
Drawings
FIG. 1 is a flow chart of the production process according to the present invention;
FIG. 2 is a diagram of a layer structure;
FIG. 3 shows phase diffraction peaks for the coating;
FIG. 4 is a graph of oxidation time versus weight gain.
Detailed Description
Example 1: oxidation-resistant molybdenum protection tube for producing phi 8 x 1 x 500mm thermocouple
Referring to fig. 1:
1. placing the inner surface and the outer surface of a molybdenum tube in a 5 wt% NaOH solution, and ultrasonically cleaning for 20min at room temperature to remove surface oxides; then, the pipe is ultrasonically cleaned by alcohol and distilled water and is dried in an oven at the temperature of 80 ℃.
2. And (3) placing a molybdenum block with the diameter of 6 multiplied by 4mm at one end of a molybdenum tube, and performing end socket welding by using argon arc welding, wherein the welding current is 100A, and the argon flow is 15 ml/min. And (3) after welding, the molybdenum tube with the blind end is cleaned by repeating the method in the step (1), dried for later use, and the surface oxide at the welding position is cleaned to obtain a matrix to be infiltrated.
Ti powder (by weight) and SiO2Powder (weight), NH4F (volume) is mixed according to 40:50:10, Ti powder needs 160.8g, SiO2The powder needs 201g, NH4F is 40.2 g. Mixing the powder materials and performing ball milling for 2 hours in a ball milling tank to obtain infiltration powder materials 1 for later use.
Calculating the total mass m of the powder to be infiltrated 2 according to the methodInner part≥0.18×94.5＝17.02g，mOuter coverNot less than 2.5 × 126.1 ≥ 315.3 g. Therefore, the total mass of the infiltration powder 2 is about 333 g. Wherein the Ti powder needs 133.2g, SiO2166.5g of powder, NH4F is 33.3 g. And mixing the powder materials and performing ball milling for 2 hours in a ball milling tank to obtain infiltration powder materials 2 for later use.
4. Calculating the total mass of the mixture:
the internal and external surface areas of the molybdenum protection tube are as follows:
internal surface area
External surface area
Wherein d is the outer diameter of the protective tube, k is the wall thickness, and L is the length of the protective tube, wherein the thickness of the molybdenum block and the surface area change caused by the blind end after welding are ignored.
Calculated from the above formula, SInner part＝94.5cm2，SOuter cover＝126.1cm2。
The total mass m of the mixture is more than or equal to m0·SInner part+m1SOuter cover，
In the formula, m0、m1For the permeability coefficient, the matrix sheet is expressedMass of mixture required for specific surface area, outer surface m1＝3g/cm2Inner surface m0＝0.24g/cm2，SInner part、SOuter coverRespectively the inner and outer surface areas of the substrate contacting with the embedded infiltration material.
Calculating the total mass m of the mixed powder needing to be filled of the powder 1 to be infiltratedInner part≥0.24×94.5＝22.7g，mOuter cover378.5 g. Therefore, the total mass of the powder 1 to be infiltrated is about 402 g.
Injecting the powder 1 to be infiltrated into the tube by using a feeding needle, placing the tube into an alumina crucible, adding the powder 1 to be infiltrated into the crucible, and completely burying the powder 1 to be infiltrated. The alumina crucible was capped with an alumina cap and sealed with a silica sol adhesive. The crucible was placed in a tube furnace and argon gas (purity: 99.999%, flow rate 30ml/min) was introduced. When the argon atmosphere in the furnace is established, the temperature is raised to 1000 ℃, the temperature is kept for 5 hours, and then the furnace is cooled to the room temperature. And (3) performing surface treatment on the pipe subjected to the embedding heat treatment 1. And (3) extracting powder in the pipe by using a feeding needle, immersing the pipe into an alcohol solution, carrying out ultrasonic cleaning on the pipe to remove embedded seeping material residues attached to the surface, and then drying the pipe in an oven at 80 ℃.
Injecting the powder 2 to be infiltrated into the tube by using a feeding needle, placing the tube into an alumina crucible, adding the powder 2 to be infiltrated into the crucible, and completely burying the powder 2 to be infiltrated. The crucible was placed in a tube furnace and argon gas (purity: 99.999%, flow rate 30ml/min) was introduced. When the argon atmosphere in the furnace is established, the temperature is raised to 1100 ℃, the temperature is kept for 5 hours, and then the furnace is cooled to the room temperature. And (3) extracting powder in the pipe by using a feeding needle, immersing the pipe into an alcohol solution, carrying out ultrasonic cleaning on the pipe to remove embedded seeping material residues attached to the surface, and then drying the pipe in an oven at 80 ℃. Thus obtaining the oxidation-resistant molybdenum protection tube for the thermocouple with the diameter of 8 multiplied by 1 multiplied by 500 mm.
The molybdenum tubes of examples 2 to 4 were used to prepare antioxidant molybdenum protection tubes for thermocouples as described in example 1, and the relevant parameters were set as follows.
The following experiments were carried out using the protective tubes prepared in examples 1 to 4:
1. sampling the cross section of the molybdenum protection tube after the buried infiltration treatment, observing the phase difference between the surface of the coating and the cross section by using a scanning electron microscope back scattering electron signal (BSE), and recording the thickness of each layer. The results are shown in FIG. 2.
2. The coating surface phase was analyzed by an X-ray powder diffractometer, and the results are shown in fig. 3. The test adopts CuK alpha rays, tube voltage of 40kV, tube current of 30mA, scanning range of 10-80 degrees and scanning speed of 3 degrees/min.
3. According to GB/T13303-91 method for measuring oxidation resistance of steel and HB5258-2000 method for measuring oxidation resistance of steel and high-temperature alloy, the oxidation resistance of a molybdenum alloy pipe sample with a coating under a high-temperature oxidation environment of 1200 ℃ is recorded. And (3) putting the sample into a crucible in a box-type resistance furnace by adopting a cyclic oxidation method, quickly heating the sample from room temperature to 1200 ℃, preserving the temperature for 10 hours, taking out the crucible, and cooling the crucible to room temperature. This is denoted as an oxidation cycle. The mass change of the sample was measured for each oxidation cycle, and the mass change per unit area Δ G of the sample was plotted against the oxidation time t, with the results shown in fig. 4. The calculation formula of Δ G is shown below. And when the delta G is less than or equal to 0, the oxidation time is the cyclic oxidation life of the coating.
In the formula: m isiThe mass of the sample after the ith oxidation cycle, mg; m is0Mg is the mass of the sample before oxidation; s is the sample surface area, cm2。
And (4) conclusion:
1. (Mo, Ti) Si continuously distributed in the coating outer layer with the diameter of about 10 mu m2The second outer layer is MoSi with a thickness of about 45 μm2Layer, between coating and substrate, of Mo of about 10 μm thickness5Si3A transition layer;
2. the outer surface of the coating is made of MoSi2With (Mo, Ti) Si2Two phases are formed;
3. whole coatingThe layer is (Mo, Ti) Si2-MoSi2-Mo5Si3The molybdenum protection tube with the composite coating is continuously oxidized for 180 hours under the periodic cyclic oxidation environment of 1200 ℃, and no obvious weight loss occurs, which shows that the coating has obvious anti-oxidation effect on the molybdenum and the alloy protection tube thereof.
The technological parameters for producing the molybdenum protection tubes with other specifications are shown in the following table:
TABLE 1 molybdenum tube Specifications and related parameters
Claims (5)
1. A method for preparing an antioxidant coating on the surface of a molybdenum and molybdenum alloy protection tube is characterized by comprising the following steps:
1) cleaning of
Putting the protection tube into 5 wt% NaOH solution, ultrasonically cleaning, then ultrasonically cleaning the protection tube in alcohol and distilled water in sequence, and drying;
2) end enclosure treatment of protective tube
Welding one end of the protection tube by using cylindrical molybdenum block argon arc welding, and then cleaning by using the method in the step 1) to obtain a matrix to be infiltrated;
3) preparation of the powder to be infiltrated 1
According to the proportion of Ti powder: SiO 22Powder: NH (NH)4F, preparing materials according to the weight ratio of 40:50:10, and carrying out ball milling and mixing for 2 hours to obtain powder to be infiltrated 1;
wherein the total mass m of the mixture is more than or equal to m0·SInner part+m1SOuter cover，
In the formula m0、m1Is buried permeability coefficient, outer surface m1＝3g/cm2Inner surface m0＝0.24g/cm2，SInner part、SOuter coverThe inner and outer surface areas of the substrate contacted with the embedded seeping material respectively;
4) heat treatment for infiltration into earth 1
Injecting the powder 1 to be infiltrated into a protective tube, placing the protective tube in a crucible, embedding the powder 1 to be infiltrated, sealing the crucible, heating to 900-1100 ℃ under the argon condition, preserving the heat for 1-9 hours, and then cooling to room temperature to obtain an outer coating layer;
5) surface treatment of pipes
Taking out the powder in the protection tube, immersing the protection tube in an alcohol solution, and drying after ultrasonic cleaning;
6) preparation of the powder to be infiltrated 2
According to Si powder: SiO 22Powder: NH (NH)4F, preparing materials according to the weight ratio of 40:50:10, and carrying out ball milling and mixing for 2 hours to obtain powder 2 to be infiltrated;
wherein the total mass of the mixture of the powder 2 to be infiltrated meets the condition that m is more than or equal to m0·SInner part+m1SOuter cover，
In the formula, m0、m1Is buried permeability coefficient, outer surface m1＝2.5g/cm2Inner surface m0＝0.18g/cm2，SInner part、SOuter coverThe inner and outer surface areas of the substrate contacted with the embedded seeping material respectively;
7) burying and infiltrating heat treatment 2
Repeating the step 4), wherein under the argon condition, the temperature is increased to 900-1300 ℃, the temperature is kept for 1-9 h, and then the coating is cooled to room temperature to obtain a secondary coating layer;
repeat step 5).
2. The method of claim 1, wherein: the outer layer of the coating is (Mo, Ti) Si2Layer, the secondary outer layer is MoSi2Mo is between the layer, the coating and the substrate5Si3And a transition layer.
3. The method of claim 2, wherein: the thickness of the outer layer is 5-20 mu m, the thickness of the secondary outer layer is 40-70 mu m, and the thickness of the transition layer is 5-30 mu m.
4. The method of claim 1, wherein: the molybdenum block in the step 2) is a cylindrical molybdenum block with the same inner diameter as the pipe.
5. The method of claim 1, wherein: the welding current in the step 2) is 50-150A, and the argon flow is 15 ml/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113025951A (en) * | 2021-03-02 | 2021-06-25 | 南昌大学 | Molybdenum alloy containing antioxidant composite coating and preparation method thereof |
| CN113025951B (en) * | 2021-03-02 | 2022-06-07 | 南昌大学 | Molybdenum alloy containing antioxidant composite coating and preparation method thereof |
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